Abstract
A simple, rapid, sensitive procedure based on solid-phase disk extraction (SPDE) is described for the isolation and concentration of trace levels of selected organochlorine pesticides from human body fluids (serum, cord blood, milk, follicular and seminal fluid). Similar methodology can be used for each matrix; the only restricting factor is the viscosity of the fluid. After denaturizing proteins with formic acid, an Empore™ C18-bonded silica extraction disk cartridge is used for the extraction of the analytes. Subsequent cleanup and lipid removal from the SPDE eluate is achieved by adsorption chromatography on acidified silica or Florisil, depending on the interest in acid-labile pesticides. By using the SPDE procedure, high-throughput parallel-sample processing can be achieved. Instrumental analysis is done by gas chromatography-mass spectrometry in electron-capture negative ionization mode (GC-MS/ECNI). Recoveries for selected organochlorine pesticides range from 65 to 91% (SD <10%) for serum and from 70 to 102% (SD <14%) for milk. Detection limits between 10 and 100 pg/mL fluid can be obtained. The method was validated through successful participation in several interlaboratory tests and through the routine analysis of human serum with various loadings of organochlorine pesticides.
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References
Simonich, S. L., and Hites, R. A. (1995) Global distribution of persistent organochlorine compounds. Science 269, 1851–1854.
Colosio, C., Tiramani, M., and Maroni, M. (2003) Neurobehavioral effects of pesticides: state of the art. Neurotoxicology 24, 577–591.
Fleeger, J. W., Carman, K. R., and Nisbet, R. M. (2003) Indirect effects of contaminants in aquatic ecosystems. Sci. Total Environ. 317, 207–233.
Greizerstein, H. B., Gigliotti, P., Vena, J., Freudenheim, J., and Kostyniak, P.J. (1997) Standardization of a method for the routine analysis of PCB congeners and selected pesticides in human serum and milk. J. Anal. Toxicol. 21, 558-566.
Najam, A. R., Korver, M. P., Williams, C. C., Burse, V. W., and Needham, L. L. (1999) Analysis of a mixture of PCBs and chlorinated pesticides in human serum by column fractionation and dual-column capillary gas chromatography with ECD. J. AOAC Int. 82, 177–185.
Mañes, J., Font, G., and Pico, Y. (1993) Evaluation of a SPE system for determining pesticide residues in milk. J. Chromatogr. 642, 195–204.
Dmitrovic, J., Chan, S. C., and Chan, S. H. Y. (2002) Analysis of pesticides and PCB congeners in serum by GC/MS and SPE cleanup. Toxicol. Lett. 134, 253–258.
Barr, J. R., Maggio, V. L., Barr, D. B., et al. (2003) New high-resolution mass spectrometric approach for the measurement of polychlorinated biphenyls and organochlorine pesticides in humans serum. J. Chromatogr. B 794, 137–148.
Pitarch, E., Serrano, R., Lopez, F. J., and Hernandez, F. (2003) Rapid multiresidue determination of organochlorine and organophosphorus compounds in human serum by solidphase extraction and gas chromatography coupled to tandem mass spectrometry. Anal. Bioanal. Chem. 376, 189–197.
Sandau, C. D., Sjödin, A., Davis, M. D., et al. (2003) Comprehensive solid-phase extraction method for persistent organic pollutants. Validation and application to the analysis of persistent chlorinated pesticides. Anal. Chem. 75, 71–77.
Pauwels, A., Wells, D. A., Covaci, A., and Schepens, P. (1998) Improved sample preparation method for selected persistent organochlorine pollutants in human serum using solidphase disk extraction with gas chromatographic analysis. J. Chromatogr. B 723, 117–125.
Covaci, A. and Schepens, P. (2001) Improved determination of selected POPs in human serum by solid phase disk extraction and GC-MS. Chemosphere 43, 439–447.
Covaci, A. and Schepens, P. (2001) Solid phase disk extraction method for the determination of POPs form human body fluids. Anal. Lett. 34, 1449–1460.
Pauwels, A., Covaci, A., Delbeke, L., Punjabi, U., and Schepens, P. (1999) The relation between levels of selected PCB congeners in human serum and follicular fluid. Chemosphere 39, 2433–2441.
Covaci, A., Hura, C., and Schepens, P. (2001) Solid phase disk extraction: an improved method for determination of organochlorine residues in milk. Chromatographia 54, 247–252.
Covaci, A., Jorens, P., Jacquemyn, Y., and Schepens, P. (2002) Distribution of PCBs and organochlorine pesticides in umbilical cord and maternal serum. Sci. Total Environ. 298, 45–53.
Koppen, G., Covaci, A., Van Cleuvenbergen, R., et al. (2002) Persistent organochlorine pollutants in human serum of 50-65 years old women in the Flanders Environmental and Health Study (FLEHS). Part 1: Concentrations and regional differences. Chemosphere 48, 811–825.
Covaci, A., Koppen, G., Van Cleuvenbergen, R., et al. (2002) Persistent organochlorine pollutants in human serum of 50–65 years old women in the Flanders Environmental and Health Study (FLEHS). Part 2: Correlations among PCBs, PCDD/PCDFs and the use of predictive markers. Chemosphere 48, 827–832.
Manirakiza, P., Covaci, A., and Schepens, P. (2002) Improved analytical procedure for determination of chlorinated pesticide residues in human serum using solid phase disc extraction (SPDE), single-step clean-up and gas chromatography. Chromatographia 55, 353–359.
Bernal, J. L., Del Nozal, M. J., and Jiménez, J. J. (1992) Some observations on clean-up procedures using sulphuric acid and Florisil. J. Chromatogr. 607, 303–309.
Massart, D. L., Vandeginste, B. G. M., Buydens, L. M. C., De Jong, S., Lewi, P. J., and Smeyers-Verbeke, J. (1997) Handbook of chemometrics and qualimetrics: Part A. Elsevier, Amsterdam.
Luotamo, M. and Aitio, A. (1997) Quality assurance of isomer-specific analysis of PCBs in serum. Chemosphere 34, 965–973.
Frame, G. M. (1997) A collaborative study of 209 PCB congeners and 6 Aroclors on 20 different HRGC columns. Fresenius J. Anal. Chem. 357, 701–722.
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Covaci, A. (2006). Application of Solid-Phase Disk Extraction Combined With Gas Chromatographic Techniques for Determination of Organochlorine Pesticides in Human Body Fluids. In: Martínez Vidal, J.L., Frenich, A.G. (eds) Pesticide Protocols. Methods in Biotechnology, vol 19. Humana Press. https://doi.org/10.1385/1-59259-929-X:049
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DOI: https://doi.org/10.1385/1-59259-929-X:049
Publisher Name: Humana Press
Print ISBN: 978-1-58829-410-4
Online ISBN: 978-1-59259-929-5
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